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WO1982002540A1 - Oxydation par voie humide de matieres organiques - Google Patents

Oxydation par voie humide de matieres organiques Download PDF

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Publication number
WO1982002540A1
WO1982002540A1 PCT/US1982/000063 US8200063W WO8202540A1 WO 1982002540 A1 WO1982002540 A1 WO 1982002540A1 US 8200063 W US8200063 W US 8200063W WO 8202540 A1 WO8202540 A1 WO 8202540A1
Authority
WO
WIPO (PCT)
Prior art keywords
slurry
concentrate
temperature
psi
organic matter
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/US1982/000063
Other languages
English (en)
Inventor
Inc Amax
Paul B Queneau
Leo W Beckstead
Robert F Hogsett
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Cyprus Amax Minerals Co
Original Assignee
Amax Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Amax Inc filed Critical Amax Inc
Priority to AT82900727T priority Critical patent/ATE15788T1/de
Publication of WO1982002540A1 publication Critical patent/WO1982002540A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/30—Obtaining chromium, molybdenum or tungsten
    • C22B34/36—Obtaining tungsten
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/005—Preliminary treatment of scrap
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the present invention relates to the treatment of oxide ores and oxide ore concentrates and, more particularly, to the wet oxidation of oxide ores and oxide concentrates.
  • the process in accordance with the present invention can be used to condition oxide ore or concentrates containing substantial amounts of carbonaceous matter which can also contain sulfides such as iron sulfide.
  • sulfides such as iron sulfide.
  • the invention will be described in terms of treatment of tungsten concentrates, particularly s ⁇ heelite concentrates.
  • organic matter is associated with oxide concentrates.
  • the concentrate can contain substantial amount of flotation reagents in addition to sulfides, such as pyrrhotite, pyrite or chalcopyrite.
  • Natural organic matter, such as humus can also be present.
  • the presence of organic matter, particularly flotation reagents can interfere with subsequent hydrometallurgical processing.
  • the presence of flotation reagents can cause substantial foaming during hydrometallurgical processing. Foaming can lower the capacity of the processing vessels, or can cause hazardous conditions by overflowing such vessels. If the flotation reagents are carried on to subsequent process steps, such as solvent extraction, the flotation reagents can contaminate the organic phase causing substantial processing inefficiencies and often requiring periodic replacement of the organic extractant.
  • the present invention relates to a process for conditioning an oxide ore or concentrate containing carbonaceous material.
  • a slurry of the oxide material and water is established in an autoclave, and the slurry is heated to a temperature of at least about 230oC under an oxygen partial pressure of at least about 25 pounds per square inch (psi) to oxidize substantially all the carbon in the material to carbon dioxide.
  • psi pounds per square inch
  • organic matter and sulfides associated with scheelite concentrate are oxidized during digestion of the scheelite concentrates with sodium carbonate solutions.
  • a slurry of scheelite concentrate in an aqueous sodium carbonate solution of an initial concentration ranging from about 50 grams per liter (gpl) to about 200 gpl at a Na 2 CO 3 : WO 3 weight ratio of between about 0.9 to about 1.6 or even higher is established in an autoclave.
  • the slurry is then heated to a temperature between about 230°C and about 320°C under an oxygen partial pressure of at least about 25 psi to digest the tungsten values content in the concentrate and to oxidize any organic matter and sulfides.
  • Scheelite concentrates which can be treated by the process in accordance with the present invention can be obtained by conventional flotation and gravity separation techniques.
  • Tungsten concentrates obtained by these methods generally contain, by weight, between about 10% and about 70% tungsten (WO 3 ), sulfides in an amount up to about 10%, generally between about 0.2% and about 1%, silica in amounts between about 2% and about 30%, ⁇ alcite in amounts between about 10% and about 70%.
  • the sulfides are present as pyrites, pyrrohtite, arsenopyrite and chalcopyrite.
  • the scheelite and wolframite concentrates can typically contain between about 0.5% and about 1% flotation oils and most frequently, between about 0.1% and about 0.2%.
  • Scheelite concentrates are slurried with water in an autoclave to provide a slurry containing between about 10% and about 75% solids, by weight, and most advantageously between about 25% and about 50% solids.
  • the slurry is heated to a temperature of at least about 230°C under an oxygen partial pressure of at least about 25 psi atmospheres to oxidize substantially all the flotation oils associated with the tungsten concentrate.
  • An important aspect of the present invention is the temperature to which the slurry of water and tungsten-bearing material is heated. At temperatures below about 230°C, the temperature is too low to be effective in oxidizing the flotation reagents at commercially acceptable rates.
  • the flotation reagents do not have to be completely oxidized to carbon dioxide and water but can be partially oxidized to shorter carbon chain products, such as acetic acid, which are compatible with digestion and downstream process requirements.
  • the process in accordance with the present invention can be conducted at any temperature lower than the critical temperature of water.
  • oxidation of the flotation oils is conducted at a temperature between about 250°C and about 290°C.
  • oxygen partial pressure over the slurry of the tungsten concentrate is the oxygen partial pressure over the slurry of the tungsten concentrate.
  • Oxygen partial pressures below about 25 psi result in the incomplete oxidation of the flotation oils or any other organic materials oxidized with the concentrate and can also result in longer reaction times.
  • Oxygen partial pressures in excess of about 800 psi can also be employed but again such high pressures require the use of extra heavy materials in construction of the autoclave thereby rendering the overall process less economically feasible.
  • oxygen partial pressure between about 100 psi and about 300 psi are employed. It will be recognized by those skilled in the art that under these conditions the total pressure in the autoclave will vary between about 400 psig and about 3,000 psig.
  • Mass transfer of oxygen from the gaseous phase to the aqueous phase and between the aqueous phase and the solids is facilitated by agitation of the heated slurry with conventional mixers in order to maintain the tungsten concentrate in suspension and to draw oxygen into the aqueous phase from the gaseous phase. Agitation is also effective in facilitating mass transfer of carbon dioxide from the aqueous phase thereby increasing the rate of oxidation by minimizing the concentration of one of the products of the reaction.
  • the process in accordance with the present invention is also effective in oxidizing any sulfides contained in the ore or ore concentrate.
  • the oxidation of such sulfides is advantageous in that the sulfide sulfur is not transferred with subsequent process operations.
  • the oxidation of the sulfides can produce sulfuric acid which can consume reagents, such as sodium carbonate or sodium hydroxide, in subsequent processing of tungsten concentrates, this adverse effect can be minimized by employing sufficient additional amounts of the reagent to react with the sulfuric acid.
  • An advantageous feature of the present invention is that oxidation of the flotation reagent and sulfides generates heat which offsets external process heat requirements for maintaining the process temperatures. Indeed, this process could conceivably generate excess heat which can be utilized in subsequent operations or for the generation of power.
  • an advantageous embodiment of the present invention is the oxidation of organic matter and sulfides associated with scheelite concentrates during digestion with sodium carbonate solutions.
  • wolframite concentrates can be treated in a like manner, except the wolframite is digested with sodium hydroxide.
  • Mixtures of scheelite and wolframite can be treated as described in copending application.
  • the invention provides an improved process for the soda ash (Na 2 CO 3 ) digestion of low-grade scheelite concentrates, particularly low-grade scheelite concentrates containing about 2% to 40% WO 3 , generally about 5% to 30% WO 3 , e.g., about 10% to 20%.
  • the process is based on the discovery of a surprising interaction between soda ash concentration, the Na 2 CO 3 /WO 3 weight ratio, the aqueous tungsten concentration in the pregnant liquor, and the temperature employed in the digestion of scheelite concentrates in aqueous soda ash solution.
  • the recognition of the interrelationships between the aforementioned four parameters has enabled the substantial reduction in the amount of soda ash required to attain the desired tungsten extraction, has minimized the excess soda ash in the pregnant liquor, and has provided maximum yield of the tungsten while minimizing dissolution of gangue minerals.
  • the maintenance of a low quantity of soda ash in the autoclave discharge pregnant liquor is important in that as the quantity of soda ash discharge increases, so does the subsequent sulfuric acid demand, the volume of gas to be scrubbed during MoS 3 precipitation and also the amount of sodium sulfate in the solvent extraction raffinate.
  • One embodiment of the invention comprises forming a slurry of scheelite concentrate in an aquous sodium carbonate solution of initial concentration ranging from about 50 gpl to 200 gpl (grams per liter) at a relatively low Na 2 CO 3 /WO 3 weight ratio of about 0.9 to 1.6 or higher and then digesting said slurry in an autoclave at an elevated temperature ranging from about 230°C to 320°C, e.g., about 250 °C to about 290°C under an oxygen partial pressure of at least about 25 psi.
  • the scheelite concentrate contains substantial amounts of sulfide minerals, greater amounts of sodium carbonate may have to be employed to insure high tungstate extraction because the sulfides upon oxidation produce sulfates which during digestion react with the sodium carbonate to form sodium sulfate thereby lowering the amount of sodium carbonate available for digesting tungsten values.
  • Improved process efficiency is obtained by employing the Na 2 CO 3 concentration of the leach solution in substantially inverse relationship with the digestion temperature and in substantially direct relationship with the Na 2 CO 3 /WO 3 weight ratio, the relationship selected being such as to effect the consistent dissolution of at least about 95% of the WO 3 in the concentrate, preferably at least about 99%, and provide a pregnant liquor containing said WO 3 .
  • the soda ash concentration range from about 75 gpl to 175 gpl and, more preferably, from about 75 gpl to 150 gpl.
  • the Na 2 CO 3 /WO 3 weight ratio may range from about 1 to 1.4.
  • the improved process is particularly applicable to the soda ash pressure digestion of difficult-to-leach low-grade scheelite concentrates containing by weight at least about 2% and preferably from about 5% to 30% WO 3 .
  • the invention is applicable to scheelite concentrates containing about 2% to 70% WO 3 .
  • Such concentrates generally contain at least about 2% silica and up to about 30% CaCO 3 .
  • the soda ash process of the invention can result in substantially increased gangue material dissolution.
  • this effect is minimal in the soda ash process of the invention due to the decreased Na 2 CO 3 requirements at higher reaction temperatures.
  • Less Na 2 CO 3 means less alkalinity, which limits attack of concentrate gangue constituents.
  • the autoclave discharge liquor's pH is about 11.1 at 180°C, 10.7 at 200oC, and 10.5 at 230°C, due to the lower amounts of Na 2 CO 3 at the higher temperatures.
  • the Na 2 CO 3 /WO 3 ratio is advantageously controlled at about 0.9:1 to 1.6:1, preferably about 1:1 to 1.4:1.
  • the concentration of Na 2 WO 4 attained in the pregnant liquor during digestion is important in providing high dissolution yields.
  • the primary digestion reaction involved both Na 2 CO 3 and Na 2 WO 4 and is reversible.
  • extraction is increased.
  • decreasing this ratio or increasing the amount of Na 2 WO 4 in the pregnant liquor will have a negative effect on the extraction efficiency.
  • the tungsten concentration constraints can be minimized by leaching to not more than about 100 gpl WO 3 , e.g., about 75 to 95 gpl, and, more preferably, over the range of approximately 90 to 95 gpl WO 3 .
  • the pregnant liquor containing the sodium tungstate is further treated following filtration to remove such impurities as molybdenum. Any excess sodium carbonate is neutralized with acid and the pH adjusted to that value required to effect precipitation of Mo as MoS 3 using sulfide ion as the precipitate. It is important that the WO 3 /Mo ratio in the purified solution be very high, for example, 20,000/1. To achieve this, the discharge pregnant solution is advantageousl0 at least about 100 gpl WO 3 .
  • One method to achieve the foregoing requirements is to leach to a final WO 3 concentration of less than 100 gpl, for example,to a range of about 75 to 95 gpl, more preferably, approximately 90 to 95 gpl, to obtain a high dissolution yield and the subject the discharge pregnant liquor to flash down to evaporate sufficient solution to increase the concentration of WO 3 in the pregnant liquor at least 10% and preferably at least about 15 or 20% of the original concentration to increase the WO 3 concentration to upwards of about 120 to 140 gp
  • fine grinding of the ore or concentrate can increase the amount of tungsten that is solubilized under a given leach condition, although fine grinding can increase substantially the amount of the water in the filter cake.
  • Concentrates having a particle size of minus 150 mesh can be treated.
  • the bulk of the material should be minus 325 mesh, with at least about 25% minus 400 mesh.
  • EXAMPLE I This example demonstrates the effects of temperature and oxygen partial pressure during the digestion of scheelite concentrates which are characterized in Table I.
  • the samples of the concentrates were slurried with water containing initially 150 gpl Na 2 CO 3 with the Na 2 CO 3 :WO 3 ratio being 1.2 to 1.
  • the slurry was fed to a two liter Parr titanium autoclave.
  • a single 5.8-cm diameter, 6-bladed axial flow radial turbine impeller located 2.5 cm off the reactor bottom was used to agitate the slurry. Heat was provided by an electric heating mantle.
  • a run was begun by adding a charge of concentrate to the reactor along with enough sodium carbonate solution to give the desired carbonate concentration and a slurry concentration of the desired percent solids.
  • the slurry was agitated at 600 rpm.
  • the slurry was then heated to the reaction temperature under the oxygen partial pressure specified in Table II. After reaching the reaction temperature shown in Table II, additional oxygen was introduced into the autoclave (if necessary) to bring the total pressure to the steam pressure plus the desired oxygen overpressure.
  • the autoclave was discharged and the slurry was filtered to obtain a pregnant liquor that was analyzed for total organic carbon (TOC) and WO 3 .
  • the solids were washed several times with the washings combined for WO 3 analysis along with the wash residue to determine tungsten extraction.
  • Reference to Table II confirms that temperatures below 250°C are ineffective in successfully reducing the total organic carbon with the result that those tests conducted at temperatures below 250°C provided a filtrate which displaced substantial foaming. Reference to Table II also confirms that high oxygen partial pressures are more effective in lowering the total organic carbon content of the filtrates and in reducing the amount of foaming the filtrate displaced upon air sparging. Reference to tests 16 through 19 also demonstrates that concentrates containing significant amounts of sulfides lower the tungsten extraction by reacting with the sodium carbonate to form sodium sulfate. With concentrates containing such high sulfide concentrations, tungsten recovery can be improved by using greater amounts of sodium carbonate.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Oxygen, Ozone, And Oxides In General (AREA)

Abstract

On forme une boue de minerai d'oxyde ou de concentre de minerai contenant de la matiere organique en les melangeant avec de l'eau et en les chauffant a une temperature d'au moins environ 230 C sous une pression partielle d'oxygene d'au moins environ 25psi pour oxyder la matiere organique. Le procede decrit dans la presente invention peut etre utilise avantageusement dans le traitement de concentres de tungstene et peut etre utilise pendant la digestion des concentres de tungstene au moyen de solutions de carbonate de sodium ou d'hydroxyde de sodium.
PCT/US1982/000063 1981-01-19 1982-01-19 Oxydation par voie humide de matieres organiques Ceased WO1982002540A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT82900727T ATE15788T1 (de) 1981-01-19 1982-01-19 Behandlung von organische bestandteile enthaltenden scheelite-zusammensetzungen.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US06/225,904 US4342728A (en) 1981-01-19 1981-01-19 Process for digesting tungsten ores containing organic matter
US225904810119 1981-01-19

Publications (1)

Publication Number Publication Date
WO1982002540A1 true WO1982002540A1 (fr) 1982-08-05

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Family Applications (1)

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PCT/US1982/000063 Ceased WO1982002540A1 (fr) 1981-01-19 1982-01-19 Oxydation par voie humide de matieres organiques

Country Status (5)

Country Link
US (1) US4342728A (fr)
EP (1) EP0069780B1 (fr)
JP (1) JPS58500022A (fr)
CA (2) CA1183003A (fr)
WO (1) WO1982002540A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2567869A1 (fr) * 1984-07-18 1986-01-24 Daicel Chem Procede de recuperation de composes de tungstene
CN111424170A (zh) * 2019-04-22 2020-07-17 中国科学院过程工程研究所 一种酸性萃取生产仲钨酸铵的方法及系统
CN111424174A (zh) * 2019-04-22 2020-07-17 中国科学院过程工程研究所 一种去除金属原料浸出液中表面活性剂的方法、净化装置及用途

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4504448A (en) * 1984-02-27 1985-03-12 Amax Inc. Activated carbon adsorption of flotation reagents from tungsten solutions
CN106379941B (zh) * 2016-10-12 2017-08-04 佛山迅拓奥科技有限公司 一种高纯度三氧化钨的制备方法

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB459554A (en) * 1935-08-24 1937-01-11 Int Hydrogenation Patents Co Process for the working up of materials containing molybdenum or tungsten
US2187750A (en) * 1936-07-31 1940-01-23 Marvin Metals Inc Treatment of ores
US2351678A (en) * 1943-11-03 1944-06-20 Robert G Hall Process for the recovery of tungsten from its ores
US3429693A (en) * 1965-12-27 1969-02-25 Fmc Corp Extraction of metals
US3656888A (en) * 1969-10-02 1972-04-18 American Metal Climax Inc Liquid phase oxidation process
US3714325A (en) * 1970-11-17 1973-01-30 Us Interior Recovery of molybdenite
US4165362A (en) * 1977-04-08 1979-08-21 Engelhard Minerals & Chemicals Corporation Hydrometallurgical processing of molybdenite ore concentrates
US4167555A (en) * 1978-06-05 1979-09-11 The United States Of America As Represented By The Secretary Of The Interior Extraction of tungsten from ores

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB459554A (en) * 1935-08-24 1937-01-11 Int Hydrogenation Patents Co Process for the working up of materials containing molybdenum or tungsten
US2187750A (en) * 1936-07-31 1940-01-23 Marvin Metals Inc Treatment of ores
US2351678A (en) * 1943-11-03 1944-06-20 Robert G Hall Process for the recovery of tungsten from its ores
US3429693A (en) * 1965-12-27 1969-02-25 Fmc Corp Extraction of metals
US3656888A (en) * 1969-10-02 1972-04-18 American Metal Climax Inc Liquid phase oxidation process
US3714325A (en) * 1970-11-17 1973-01-30 Us Interior Recovery of molybdenite
US4165362A (en) * 1977-04-08 1979-08-21 Engelhard Minerals & Chemicals Corporation Hydrometallurgical processing of molybdenite ore concentrates
US4167555A (en) * 1978-06-05 1979-09-11 The United States Of America As Represented By The Secretary Of The Interior Extraction of tungsten from ores

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"Tungsten" published, 1979, Plenum Press, N.Y., pp. 82-83, YIK et al. *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2567869A1 (fr) * 1984-07-18 1986-01-24 Daicel Chem Procede de recuperation de composes de tungstene
CN111424170A (zh) * 2019-04-22 2020-07-17 中国科学院过程工程研究所 一种酸性萃取生产仲钨酸铵的方法及系统
CN111424174A (zh) * 2019-04-22 2020-07-17 中国科学院过程工程研究所 一种去除金属原料浸出液中表面活性剂的方法、净化装置及用途
CN111424174B (zh) * 2019-04-22 2022-03-25 中国科学院过程工程研究所 一种去除金属原料浸出液中表面活性剂的方法、净化装置及用途

Also Published As

Publication number Publication date
EP0069780B1 (fr) 1985-09-25
EP0069780A1 (fr) 1983-01-19
EP0069780A4 (fr) 1983-06-17
US4342728A (en) 1982-08-03
JPS58500022A (ja) 1983-01-06
CA1183003A (fr) 1985-02-26
CA1175239A (fr) 1984-10-02

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